Magnetic core/shell/shell triple structure material with noble metal nano particles being at double-shell interlayer and preparation method of material

A nanoparticle and triple structure technology is applied in the field of magnetic core/shell/shell triple structure materials and their preparation, which can solve the loss of metal, increase energy consumption and cost in the production process, and do not solve the problem of increasing the agglomeration of loaded nano metal particles. and other problems, to achieve the effect of preventing loss and agglomeration, and good magnetic responsiveness

Active Publication Date: 2014-10-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the magnetically supported nano-metal catalysts have solved the problem of catalyst recovery well, they have not solved the problems of agglomeration of supported nano-metal particles on the carrier and metal loss; at the same time, due to the high catalytic activity of the supported magnetic nano-metal Some multi-component reactant systems are often accompanied by the generation of many by-products when the target product is obtained, which requires additional operating procedures such as product separation and purification, thereby increasing the energy consumption and cost of the corresponding production process

Method used

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  • Magnetic core/shell/shell triple structure material with noble metal nano particles being at double-shell interlayer and preparation method of material
  • Magnetic core/shell/shell triple structure material with noble metal nano particles being at double-shell interlayer and preparation method of material
  • Magnetic core/shell/shell triple structure material with noble metal nano particles being at double-shell interlayer and preparation method of material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Fe 3 o 4 SiO 2 / PdZIF-8 synthesis:

[0023] (1) Add 1.35g of ferric chloride hexahydrate and 3.6g of sodium acetate into 40mL of ethylene glycol and stir for 1h to dissolve it, then put it into a synthesis kettle at 200°C for 8h, then wash with ethanol for 3 times; then take 0.1g of Got Fe 3 o 4 Add 60mL of ethanol, 1mL of water, 2mL of ammonia water (28%) and 160μL of tetraethyl orthosilicate to the mixed solution, stir at 40°C for 6h to obtain Fe 3 o 4 SiO 2 core-shell particles.

[0024] (2) Take 15mL of 2mM H 2 PdCl 4 Add 21 mL of water, 14 mL of ethanol and 0.0667 g of PVP to the mixture and reflux for 3 h to obtain PVP-Pd nanoparticles.

[0025] (3) Fe obtained from the above step (1) 3 o 4 SiO 2 Add 20mL of APTES ethanol solution with a concentration of 1% by mass to the core-shell particles and stir mechanically at 60°C for 8h, and then the treated Fe 3 o 4 SiO 2 Add 10 mL of the PVP-Pd nanoparticle solution with a mass percent concentration of 0...

Embodiment 2

[0028] Fe 3 o 4 SiO 2 / PtZIF-8 synthesis:

[0029] (1) 5 mL of K at a concentration of 10 mM 2 PtCl 4 Add the solution to a mixture of 12.5 mL of 0.4 M TTAB and 29.5 mL of water, stir for 15 minutes, add 3 mL of 0.5 M sodium borohydride aqueous solution, and continue stirring at 50 ° C for 15 h to obtain TTAB - Pt nanoparticles.

[0030] (2) the Fe processed with APTES prepared in Example 1 3 o 4 SiO 2 Add 10 mL of the TTAB-Pt solution with a mass percent concentration of 0.001% synthesized in the above step (1) to the core-shell particles, and stir at 60° C. for 1 h.

[0031] (3) Add the magnetic particles obtained in the above step (2) directly to a mixture of 0.16 g of zinc nitrate dihydrate, 0.4 g of 2-methylimidazole, and 20 mL of methanol, and stir at 30° C. for 4 h to obtain Fe 3 o 4 SiO 2 / PtZIF-8 core / shell / shell particles.

Embodiment 3

[0033] Fe 3 o 4 SiO 2 / AuZIF-8 synthesis:

[0034] (1) 5 mL of 38.8 mM sodium citrate aqueous solution was quickly added to 50 mL of 1 mM HAuCl 4 solution, and then stirred and refluxed for 15 minutes to obtain citrate-protected Au nanoparticles.

[0035] (2) the Fe processed with APTES prepared in Example 1 3 o 4 SiO 2 Add 10 mL of the Au nanoparticle solution with a mass percent concentration of 0.001% synthesized in the above step (1) to the particles, and stir at 60° C. for 1 h.

[0036] (3) Add the magnetic particles obtained in the above step (2) directly to a mixture of 0.16 g of zinc nitrate dihydrate, 0.4 g of 2-methylimidazole, and 20 mL of methanol, and stir at 30° C. for 4 h to obtain Fe 3 o 4 SiO 2 / AuZIF-8 core / shell / shell particles.

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Abstract

The invention belongs to the field of magnetic materials and relates to a magnetic core/shell/shell triple structure material with noble metal nano particles being at a double-shell interlayer and a preparation method of the material. The preparation method comprises the following steps: with Fe3O4 magnetic particles as a core, performing surface hydrolysis on the magnetic particles through hydrolyzing tetraethyl to form a layer of SiO2, then loading the noble metal nano particles with catalytic activity on the SiO2 by a coupling method, and finally coating with a ZIF-8 shell layer with regular pore channels to enable the noble metal nano particles to be positioned at the double-shell interlayer, thus obtaining the magnetic core/shell/shell triple structure material. The obtained composite material has the advantages that not only can fast separation of the material and a reaction system be realized by adding a magnetic field, but also the noble metal nano particles are positioned at the double-shell interlayer to be prevented from being lost and gathered, and simultaneously the ZIF-8 membrane layer with micropores at the outer layer also can endow the material with shape-selective and selectively-permeable functions, so that the magnetic core/shell/shell triple structure material has good potential application prospect in the fields of shape-selective adsorption and catalysis.

Description

technical field [0001] The invention belongs to the field of magnetic materials, and in particular relates to a magnetic core / shell / shell triple structure material with noble metal nanoparticles in a double-shell interlayer and a preparation method thereof. technical background [0002] Nano-noble metal particles represented by Pd, Pt, and Au are widely used in catalytic fields such as oil refining, petrochemical industry, and organic synthesis due to their large specific surface area, high catalytic activity, and reaction selectivity, such as hydrogenation reactions. Sexual hydrogenation can make unsaturated alkenes and alkynes into saturated alkanes, make unsaturated alcohols, aldehydes, ketones, and acids into saturated organic substances, and make liquid oils become solid after hydrogenation; selective oxidation production in oxidation reaction Acetaldehyde, vinyl acetate, methyl methacrylate; and carbon-carbon coupling reactions of aromatic compounds with organic halide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J33/00B01J35/02
Inventor 张雄福张通严心涓刘海鸥邱介山
Owner DALIAN UNIV OF TECH
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